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A kind of synthesis method of guanidine organic magnetic ionic liquid and its use in constructing magnetic two-phase system

A magnetic ionic liquid, ionic liquid technology, applied in separation methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of difficulty in two-phase separation, unfavorable mass and heat transfer, and high price, and achieve good application prospects and high cost. The effect of enrichment factor and easy operation

Active Publication Date: 2017-09-12
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this type of system include: need to use a relatively large amount of high molecular polymer, and its price is high; due to the high viscosity of high polymer aqueous solution, it is not conducive to mass transfer and heat transfer, which affects the separation rate; It is easy to emulsify during the process, which makes it difficult to separate the two phases after the extraction, etc.
So far, there has been no report on magnetic ionic liquids capable of forming aqueous two-phase systems

Method used

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  • A kind of synthesis method of guanidine organic magnetic ionic liquid and its use in constructing magnetic two-phase system
  • A kind of synthesis method of guanidine organic magnetic ionic liquid and its use in constructing magnetic two-phase system
  • A kind of synthesis method of guanidine organic magnetic ionic liquid and its use in constructing magnetic two-phase system

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Synthesis:

[0035] (1) 4-Hydroxy-2,2,6,6-tetramethylpiperidine oxide (4-OH-tempo) was dissolved in chloroform, stored under ice bath conditions, and slowly added dropwise while the system was stirring Add equimolar amounts of chlorosulfonic acid to the solution; then continue to stir at room temperature for 12 hours, evaporate under reduced pressure; wash the solid product with dichloromethane, remove the organic solvent by evaporating under reduced pressure, and obtain tempo-OSO 3 H, stored under vacuum.

[0036] (2) Will work with tempo-OSO 3 H Equimolar amounts of 1,1,3,3-tetramethylguanidine (TMG) dissolved in ethanol / acetone, mixed with tempo-OSO 3 The ethanol / acetone solution of H was mixed and stirred, and the organic solution was evaporated under reduced pressure to obtain a red viscous liquid, which was the final product, which was dried and stored in vacuum.

Embodiment 2

[0038] Synthesis of 2:

[0039] (1) 4-Hydroxy-2,2,6,6-tetramethylpiperidine oxide (4-OH-tempo) was dissolved in chloroform, stored under ice bath conditions, and slowly added dropwise while the system was stirring The chlorosulfonic acid of equimolar amount was added into the solution, and the system began to precipitate solids at this time; then continued stirring at room temperature for 23 hours, and evaporated under reduced pressure; the solid product was washed with dichloromethane, and the organic solvent was removed by evaporation under reduced pressure to obtain tempo- OSO 3 H, stored under vacuum.

[0040] (2) Will work with tempo-OSO 3 H Equimolar amounts of 1,1,3,3-tetramethylguanidine (TMG) dissolved in ethanol / acetone, mixed with tempo-OSO 3 The ethanol / acetone solution of H was mixed and stirred, and the organic solution was evaporated under reduced pressure to obtain a red viscous liquid, which was the final product, which was dried and stored in vacuum.

Embodiment 3

[0042] Synthesis:

[0043] (1) 4-Hydroxy-2,2,6,6-tetramethylpiperidine oxide was dissolved in chloroform, stored in ice bath, and an equimolar amount of chlorine was slowly added dropwise while the system was stirring. Sulfonic acid was added to the solution, and the system began to precipitate solids at this time; the system continued to stir for 12 hours at room temperature, and evaporated under reduced pressure; the solid product was washed with dichloromethane, evaporated under reduced pressure to remove the organic solvent, dissolved in ethanol / acetone, added, etc. Molar amount of NaOH ethanol solution, the organic solvent was removed by evaporation under reduced pressure, and the crude product was dissolved in acetone for recrystallization to obtain tempo-OSO 3 Na, the product was filtered and stored in vacuum.

[0044] (2) Dissolve 1,1,3,3-tetramethylguanidine (TMG) in ethanol, add equimolar amount of ethyl bromide, stir and reflux at 70°C for 13 hours; evaporate und...

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Abstract

The invention discloses a synthesis method of guanidine organic magnetic ionic liquid, in particular guanidyl cation-based organic magnetic ionic liquid. The synthesis method is technically characterized in that chloroalkane or bromoalkane, 1,1,3,3-tetramethyl guanidine, sodium hydroxide or potassium hydroxide, a 4-hydroxy-2,2,6,6-tetramethyl piperidine oxide and chlorosulfonic acid are used as raw materials to synthesize a series of paramagnetic organic magnetic ionic liquid, and the structural formula is as shown in formula (I) shown in the description. The compound is novel in structure and can form aqueous two phase with inorganic salt (potassium phosphate, dipotassium phosphate, potassium carbonate, sodium carbonate, ammonium bisulfate, sodium sulfate and the like); an aqueous two phase system of the magnetic ionic liquid is internationally developed for the first time. Compared with the traditional aqueous two phase system, the aqueous two phase system of the magnetic ionic liquid is capable of accelerating the separation of two phases through an applied magnetic field assisted manner, so as to improve the phase separation efficiency. The system has wide potential purposes, and has unique advantage in the fields of extraction, micro-extraction, separation and analysis.

Description

technical field [0001] The invention relates to a preparation method of an organic magnetic ionic liquid and its use in constructing a magnetic two-phase system. This type of magnetic ionic liquid is different from conventional iron-containing magnetic ionic liquids, and does not contain any metal elements in its molecular structure, and can The invention forms a two-phase system, which belongs to the technical field of novel two-phase separation. Background technique [0002] As an emerging green solvent, ionic liquid has a wide range of liquids compared with traditional organic solvents; from below or close to room temperature to above 300 °C, it has high thermal and chemical stability; very small vapor pressure , non-volatile, will not evaporate during use and storage; it can be recycled, reducing environmental pollution, and has broad application prospects (Seddon K R. Ionic Liquids for Clean Technology[J].Chemical.Technology&Biotechnology, 1997, 68:351-356.). Among al...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C279/04C07C277/08C07D211/44B01D11/04
CPCB01D11/0419C07C277/08C07C279/04C07D211/44
Inventor 宋航姚田姚舜戴学志
Owner SICHUAN UNIV
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